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Dec. 1936- c. B. sAwYER El km Re- 20,214

PROCESS OF OBTAINING BERYLLIUI AND ALUMINUM COIPOUNDS Original Filed 0a. 14, 1930 :n-ncnou or 5:0 mm HEAT TREATED EXTQACTlON OF BEO FIwM RAW BEIZ1L(NEH m NEW HAMPSHIRE BERYL mo WITH suumulzlc ACID OF M-LsAMRII IAFOLY Amman VARIOUS CONCENTRATIONS qo mucnovu mo: wmv 9'91. qo W KID AV 2;- For. :5} nova;

on an a so Sen ,0 550 0 a 4 a 0 l0 l2 c.

Tm: or ngAT TREATMENT OFOEE (nouns) TEMPERATURE OF Auo TREATMENT FIG. 1 Y Fl 6 5 Bio ExTIAcTED FROM BERYL .(uzw rumvsmae 46'5t. sumwmc new AT um; FOR 14 uouas m (messuas TREATMENT) Q 7 II Eco so 3 .50

v 6.6;] FIG. 2 I 5Y2 ATTOQN EY R b at R 20,214

rosin rnocsss or on'rammo aaarmuu AND a snmmmu oourornms chariea'lflawyerandlenstliellgremcicweianll Heights, Ohio, assignorsio Them-nah Beryllium Company. Cleveland, Ohio, aeorporaticnef'ohlo Original No; 1,823,864, 15, 1931, Serial No. m, October 14, 193.. Application for reissue September 14, 1.38. Serial No. 688.496.. In Canada January 6, 1927 14 Claim (ci. zs-is) We have filed applications for patent in Canada, Serial No. 320,889, Jan. 6, i927, and in Germany. Serial No. 129.473, Jan. 31, 1927.

This invention relates to a process for the extraction of beryllium and aluminum from ores containing them, such as beryl.

Heretofore there has been -no satisfactory method of recovering beryllium from the ore beryl because of the latters extremely hlsh resistancetotheactionofmostreagents.-'

One object of this invention is to provide a method of treating beryl to make it more susceptible to the action of suitable reagents. A further object of the invention is to provide a relativelysimpie and cheap process for converting the beryllium and aluminum naturally occurring in the ore into soluble beryllium and aluminum salts from which the correspondins oxides may be formed.

Other objects of the invention will be apparent to those skilled in the m from the description of-it hereinafter given.

In describing'our process, reference will be made to the accompanying drawing which illustrates certain features of the process.

-- In the drawing, Pig. 1 is a series of curves showing the effect of heat treatment of beryl at various temperatures upon acid'recovery treatment at approximately atmospheric pressure.

Fig. 2 is a curve'and data showing the. efleet of heat treatment of beryl at various temperatures upon acid recovery treatment above atmospheric pressure.

Hg. 3 is a series of curves showing the effect of treatment under pressure of raw beryl with sulphuric acid of. various concentrations at various temperatures (pressures).

.Our invention is based primarily on the discovery that beryllium and aluminum occurring in beryl may be made susceptible to the action of suitable reagents by subjecting the beryl to the action of heat in a manner tomodify its physical structure and so render it more readily attacked by the reagent to be used. 4

The heat treatment of theberyl can be car:

ried out at various temperatures. The resulting modification of the reactivity of the ore begins at temperatures below 1000 C. and increases as the temperature of the treatment is increased. However. the increase in the efiect of the treatment with increase in the temperature of the treatment is relatively slow below 1000" C. and becomes more rapid at temperatures above 1000' C. The maximum effect is secured by heating the ore to melting, at temperatures normally minum content of the beryl.

reusing from 1500' to 1800 C.,- and such treatment renders the ore readilyattackable'by sulphuric acid. However, when the beryl is heated at the more moderatetemperature of sinterlng, such as about 1850 0., and at still lower temperatures, it is modified so that it is attacked by certain reagents, suchas sulphuric acid, although if the heat treatment of the ore is carried out at temperatures below its melting point the treat-' 1 ment generally must be continued for a longer time than when the beryl is completely melted andalsoitmaybenecessarytotreattheore at a higher temperature with the reagent if the ore hasnot beenheatedtothepointofcomplete melting. v

The modification of the reactivity of, the ore due to heating is not so pronounced if the ore is allowed to cool very slowly. Therefore, both as a matter of convenience and to secure the maximum effect of the treatment, we rapidly cool the heated ore preferably by quenching it in a suitable medium, such as water. This fixes the ore in its modified state. It is possible to cool the ore in air fairly rapidly but in order to securea maximumrateofcooling weprefertousea liquid'quenching medium. The maximum reactivity of the ore is secured by quenching it from the molten state. The effect. of quenching upon the reactivity is less if the ore is heat treated at lower temperatures.

We have foimd that beryl may be heated. as for 1 example, in. a recuperative oil fired furnace, or in an electric furnace, above the fusion point so that it forms a free flowing molten liquid and, therefore, the heating can be carried out if desired in a furnace of such character that the molten beryl will continuously run out directly into a quenching medium such as water. or if preferred, the beryl can'be melted in a furnace and poured at intervals into the quenching medium.

After modification of the beryl by any of the above methods, the beryl may be treated with a suitable reagent to attack the beryllium and alu- While it is possible to use hydrochloric acid, nitric acid, an aqueous solution of sodium hydroxide or other bases, and other reagents. to extract the aluminum and beryllium in beryl that has been modified by our improved-princess, we prefer to employ one of the mineral acids, and especially sulphuric acid, as

be .fss in mitsble rin ins m at 2 I v The. said reagent one which will render the aluminum and beryllium content of the beryl soluble in water but which will leave the silica content thereof in insoluble condition. The said reagent may be mixed with said beryl and heated to a temperature sufilciently high and for a time tly long to render said aluminum and beryllium soluble, as by the conversion thereof to soluble salts. V

It maybe noted that in general the more completely the beryl is modified, the greater is the heating and the'rapidity of the cooling connection, it may be noted that density of the beryl'appears to be an indicaof dqree of modification thereof. fl'hus, more complete the modification of the beryl,

As above indicated, we have found that sulphuric acid, preferably somewhat diluted, such as concentrations between 46 and 63 degrees Baume, is a suitable reagent-to render soluble the 1 tially atmospheric pressure. It will be understood that the reaction between the beryl and sulphuric acid may be carried out by heating the reaction mixture for longer or shorter times, de-

, pending in part upon the temperature employed.

We have discovered that the temperature and pressure at which the treatment oi the modified orewiththeacidor other reagentiscarriedout are important factors afi'ecting the degree of extraction of the beryllium and aluminum contents oftheore. Indeedtheefiectofincreasingthe -.temperatureandpressureintreatingtheorewith sulphuric acid, for example, is so marked that the treatment under pressure may under some he a major consideration in the practiceofourprocess. Purthermorawehavefound that the increased reactivity secured by treatmentunderpressureholdstrueinthecaseof. raworunheatedb'erylaswellasinthecaseof heat treated ore. Treatment of the'ore under pressure can be carried out with sulphuric acid, forsxampleinaclosedmbeononalargerscale,

in a lead lined autochve or other suitable container. Ataiaterpointinthedescriptionwe shall refer further to the treatment under pressurelnconnecflonwlththedrawing.

'By taking advantageof the differential reactemper whichthe berylhasbeenheated, the

beryLif it is desired to specially'cool th'e appears to be the density thereof. For 7 tivities of the beryllium and aluminum'com poimdsasexistinginthemodifiedberyiandof thevarkmsfaetorsaifectingtheactivltyofthe sulphuricoacidin convertingthe beryllium and aluminum ds of such be M lolllble sulphates, the beryllium and aluminum may either beextracted elyor simultaneously.asdesired. l'brexamplaifa-berylsuchasisjfoundin SouthDakotaismeltedandtreatedwithsulphuric acid of about the concentration of chamberacidandatatemperatureofabout200C.,a goodextraotionoftheberylliumfromthetreated berylisobtained, Withthesaidacidatahigher temperatm'e,suchas250' C. for instance.thealuminum isalso attacked, and it will thus be seen thatvariationofthetemperature afiords'amethod fortheseparateextraction of and aluminum contained in the original beryl. Beryis from'other deposits may have both'the beryllium content .and aluminum content renderedsoluhleevenbythefirstofthesetwotreatmentsandthereforetheamountofaetionorthe .activity ofthe acid in attacking the beryllium andaluminumcompoimdsoftheberylwillhave tobediminishedifitbc'desiredtoextractthe berylliumandaluminum auccessively,aswiilbe more fully explained. And berylsfrom still other deposits, on the other-hand, may need to have the activity of the acid increased, depending upon the composition of the beryl. The be- 'rylllumandaliuninummayeitherbeextraeted successively or simultaneously, as desired, -depending upon the desree of modification of the beryL-theconcentration of the acid used and the temperature and time of reaction between acid and the comminuted beryl. V 7

When the beryllium and aluminum contents oftheberylareattackedtoformthesolubie aluminum and beryllium sulphates, the silica is left as a'siiicic acid completely dehydrated if the temperature of treatment is sufilciently high.

The product of the reaction between the beryl and a suitable reagent. such as, for example, sul- ,phuric acid, nmybe treated; with water or other the liquid, the soluble aluminum and beryllium compounds dissolved therein, the solution filtered to remove insolublematerial and the aluminum and beryllium compoimds recovered from such filtrate, by methods hereinafter described.

Dependent on the composition of the natural beryl, there may be also considerable quantities of iron sulphate in the sulphate solution. After removing the aluminum and beryllium, a final mother liquor with the iron content therein remaim.

In carrying out our process, after treatment of themodifiedberylwithsulphuricacidweprefer toextractthesulphates with water from thesulphatedmaterialsoaatomakeanaquemusolutionoi' the sulphates; From'this solution'the aluminum sulphate may be completely separated by converting it into an alum, for example. ammonia alum, by adding a'sufilcient amount of ammonium sulphate. and subsequently removing thealumbycrystalliaation. Ithasbeenknown thatamajorportionofthealuminumcanbe separated from the other sulphates as an alum, butlmretoforeithas never been possible to secure a complete separation; According to the praentinvention a complete separation may be attainedbyeither oftwomethods,bothofwhich arebasedonthediscoverythatanalumsuch for example as ammonia alum or potassium alum,issubstantiallyinsolub leinanaoueous solutio'm'of suitable concentration and temperature,

emtainingamiatureofberyllimnmbhatoandan 1g.

alkali sulphate, such for example as ammonium sulphate or potassium sulphate.

A saturated solution of beryllium sulphate dissolves some ammonia alum at room temperature. If, however, ammonium sulphate is added the solubility of ammonia alum in this solution rapidlydecreases and is practically zero at about 18 (3., when the amount of ammonium sulphate approaches about 6% of the weight of crystalline beryllium sulphate in solution. If the beryllium sulphate solution is not saturated a greater amount of ammonium sulphate has to be added. Also if the temperature of the beryllium sulphate solution is increased, more ammonium sulphate has to be added. For practical purposes it is preferable to use an amount of ammonium sulphate equal to 10-20% of the weight of the crystalline beryllium sulphate present in order to secure a wider usable range of concentrations and temperatures.

Very high percentages of ammonium sulphate can also be used, but it is. of course, preferable to use as little ammonium sulphate as practically possible. If the amount of ammonium sulphate is less than about 6% of the weight of the crystalline beryllium sulphate the alum may still be completely separated by cooling the solution to temperatures lower than ordinary room temperatures.

One of the two separation methods referred to consists in separating the alum by adding to the.

sulphate solution obtained by leaching the sul- 'phatized ore an excess of ammonium sulphate whereby the ammonia alum formed becomes substantially insoluble in the solution and the beryllium sulphate remains entirely soluble. The exeess of ammonium sulphate used depends to some degree on the concentration of the sulphate solution. In order entirely to remove all the ammoniaalum, it is preferable to carry out the crystallization in such a way that also some beryllium sulphate is crystallized out together with the ammonia alum. After separating the ammonia alum by filtration or otherwise, the beryllium sulphate content of the alum may be washed out and the washings returned to the aqueous sulphate solution obtained from the leaching of the ore. The mother liquor obtained after separating the alum contains practically all the beryllium sulphate together with the iron content of theore. By evaporation and crystallization of the beryllium sulphate from this mother liquor most-of the iron is left in the mother liquor and a crystalline beryllium sulphat containing very little iron obtained. The other method of separating the alum consists in adding to the sulphate solution obtained by leaching the sulphated ore enough ammonium sulphate to form ammonia alum and then crystallizing out beryllium sulphate and ammonia alum together. After separation of the mixed crystals these crystals are leached with a suit-' able solution containing beryllium sulphate and ammonium sulphate. Such a leaching solution may contain, for example, 250 grams of crystalline beryllium sulphate per liter and 60 grams of ammonium sulphate per liter. A solution of this concentration is capable of extracting about 570 grams of beryllium sulphate per liter at 20 C. from a mixture of beryllium sulphate and alum without dissolving the alum. The leaching procass is carried out by stirring the mixed crystals preferably at room temperature or lower temperatures with the leaching solution. By this treatment all of the beryllium sulphate crystals left. The ammonia alum is further separatedfrom the solution by filtration or otherwise and the beryllium sulphate in the filtrate recovered by evaporation and crystallization. The remaining mother liquor containing ammonium and beryllium sulphates may then be used again for leaching purposes after proper dilution with water.

It will be seen that whichever of the two procedures for separating the alum is used there is involved essentially'the 'use of a solution of beryllium sulphate and an alkali sulphate which containsan amount of the alkali sulphate sufficient to render the alum completely insoluble in the solution of the concentration and temperature employed.

In each of the above described methods of separating the aluminum content the beryllium sulphate formed generally contains some iron. This beryllium sulphate is purified by recrystallization.

In all of the crystallizing operations herein described in whichiron is present it should preferably be in the ferrous state and such condition can be insured byany well known method, such as the introduction of sulphur dioxide or barium tration of the solution and crystallizing out of ferrous ammonium sulphate. The final mother liquor remaining from the iron crystallisation contains substantially all the excess free acid and is sufllciently reduced in iron content to permit its use as a reagent'for subsequent treatment of additional beryl, or it may be added to the sulphate solution obtained by leaching the sulphatized ore. I

If the sulphate solution obtained by leaching the ore contains much free acid, ammonia may be added insteadof ammonium sulphate. It will thus be seen that by the use of ammonia the excess sulphuric acid may be recovered as ammonium sulphate and thereby utilized in the process for the formation of ammonia alum.

The beryllium sulphate produced by our above described method can be decomposedinto sulphur trioxide and beryllium oxide by heating to tem peratures such as 800 to 1000' C. The sulphur trioxide may be converted to sulphuric acid for use in the process. Also the ammonia alum producedin the process may be decomposed into ammonium sulphate and aluminum sulphate, for

example, by the process disclosed in U. S. patent.

beryl upon the recovery of the beryllium content by our method of treatment. It will be noted that the recovery of the'beryllium content, in terms of the percent of beryllium oxide extracted, is plotted vertically against the time of the heat treatment of the beryl, the curves representing heat treatments at diiferent temperatures. The extractions oi the-modified beryl were made with 100% excess of 63' B6. sulphuric acid at 236 C. in a closed tube, the time of the acid treatment in each case being 15% hours.

It will be observed on referring to the curves that for this particular acid treatment the effect of heat treatment at 1000' C. upon the reacttivity of the beryl was measurable but .relatively small. The eilect of the heat treatment at 1200 C. is still greater but the increase is not marked. However, when the heat treatment of the beryl is carried out at 1300 C. the recovery of the beryllium content is markedly increased, being nearly double the recovery at 1200. For the heat treatment of the ore at 1400 C. the recovery in turn is iully double that for the treatment at 1300' C. The data for the treatment at 1500 C. are not so full but it will be noted that the increase in the recovery for the treatment at 1500 C. is markedly greater than that for 1400 C.; and, finally, when the ore was heated to the melting point and rapidly cooled in air the recovery was increased to about eighty percent. By quenching themelted ore in water we have been able to attain a beryllium recovery of nearly 99%.

In Fig. 2 of the drawing we present data which indicate the eil'ect both of acid treatment under pressure and of the heat treatment of the ore. This figure represents treatment of heat treated beryl with 46 Be. sulphuric acid at 251 C. (approximately 118 C. above the boiling point of the acid) for 19 hours, and the percent of beryllium oxide extracted is plotted vertically against a one-hour heat treatment of the ore at various temperatures. on comparing Fig. 2 with Fig. 1, it will be observed that the eflect of the acid treatment of the ore under pressure is to very substantially increase the extraction of beryllium oxide both from the raw ore and the heat treated ore. Even in the case of the raw ore the extraction is increased by the use of pressure from a very few percent to upwards of 50%. also, it will be seen from a comparison of these two figures that the increase in the recovery of beryllium oxide from the ore incident to the increase in the temperature of the ore treatment is even more marked when the acid treatment is carried out under substantial pressure than when it is carried out at atmospheric pressure. From Fig. 2 it will be noted that a heat treatment of the ore as low as 935 gives the relatively high extraction of beryllium oxide of76+% if the heat treatment of the ore is suiiiciently prolonged, thus bringing out the influence of the time of heat treatment of the ore.

Considering both Figs. 1 and 2, it will be seen,

eating the effect of the heat treatment of the Fig. 3 of the drawing is a series of curves representing extraction'of beryllium oxide from raw beryl by 17 hours treatment with sulphuric acid of various concentrations at various temperatures above the boiling point of the acid, the treatments being carried out in a closed container. The extraction of beryllium oxide is plotted vertically'against the temperature of the acid treatment and each curve represents a'particular acid concentration. This series of curves shows that the beryllium oxide extraction increases with decrease in the concentration of the acid and with increase in the temperature of the acid treatment, both of which factors correspond to increase in the pressure. The data in this figure also show the eflect of the time factor in the acid treatment, the extraction of beryllium ox--v ide by 46 B. acid at 265 C. being increased from about 66% to about 16% by prolonging the acid treatment from 17 hours to 46 hours.

The beryl found in different deposits varies somewhat in composition and we have found is possible, without interfering with the successful carrying out ofthe various steps of our process, to very substantially lower the melting point of the ore and thus permit a modification of the ore by our improved heat treatment at a markedly lower temperature than would otherwise be possible, thus realizing substantial economic gains in the process.

Furthermore, -.ve have found that by the addition of a suitable substance or substances it is possible to not only thus lower the melting point of the ore but also to increase the reactivity of the ore, in a manner which we do not fully understand but which we believe essentially involves a retardation of the recrystallization of the melted ore.

Among the substances which may be added to the ore for the purposes specified are compounds,

oxides for example, of iron, calcium and sodium. All of these substances when added to the ore in small amounts have the eifect of lowering its melting point and iron, for example, also has the marked added effect of increasing the reactivity of some ores when melted and quenched, this latter effect being due, we believe, to a retarding eflect upon the recrystallization of the melted ore, thus insuring the preservation to a higher degree of the modifying eflect oi the heat treatment. The addition to the ore of any one or more of the substances above mentioned obviously will not interfere with any of the several steps of our process of treatment. y

Two of the ores which we have used, one from New Hampshire and the other from South Da-' lrota, will serve to illustrate the effect of the composition of the ore which we have just been de scribing.

New Hampshire beryl South Dakota beryl Be0 ==12.s2% BeO "-12.00% 41.0 ==17.61% A120, -=17.8 9:, Fe,0, 1.26% Fe,0,. 0.61% K 0,Na,0 0.67% K,0,Nag0,Li,0 2.3 9r,

Of these two ores, that from South Dakota was from New Hampshire but the latter ore, on the other hand, after melting and rapid cooling was found to have a higher reactivity to the acid treatment. By the addition of a small amount oi iron oxide to the South Dakota ore we found it possible to increase it]! reactivity to the acid treatment, as well as to ower somewhat further its melting point, thus illustrating the efiect of modifying the composition as above described.

As illustrating the character our process we give the following specific example, in which sulphuric acid is employed as reagent:

100 lbs. of beryl, which has been melted and quenched as above explained and ground to pass a Tyler 200-mesh sieve is mixed with 120 lbs. 63' B. sulphuric acid, which is about excess of the acid. The mixture is then heated in an iron container. As soon as the acid becomes slightly warm the reaction starts, and the temperature increases rapidly. Steam and gases go omandthe mixture seems to boil. After about $6 hour the reaction slows down. The container is then covered and heated up to 250-300 C. for about 24 hours, to dehydrate the silica formed. After 'cooling, the white sulphated material is broken up in lumps and leached with water. The

insoluble residue is separated by filtration and the filtrate concentrated to a specific gravity of about 1.32 at C.

The filtrate or solution now has a volume or about 11'! "liters, and contains about:

35 grams BeO per liter 40 grams A120: per liter 3 grams FezOa per liter in the iorm'oi' sulphates.

The extracted yield oi beryllium oxide is about In order to separate the aluminum from the beryllium, ammonium sulphate is added to the solution, and ammonia alum separated by crystallization. The solution above contains 5740 grams A120: as aluminum sulphate. It would require 1400 grams ammonium sulphate to form ammonia alum. However, about excess ammonium sulphate, or 9400 grams, is used. It may be dissolved in water to a saturated solution and added directly to the cold sulphate solution. The

ammonia alum quickly and is separated by filtration.

The mother liquor has a volume or about 104 liters and a specific gravity of about 1.21 at 15' C.

It contains about:

33 gramsBeOperliter 3.2gramsAlaOaperliter 2.3gramsEeaOaperliter 10 gramstree (NHalsBOrperliter The acidity oi the solution is 0.15 to 0.20 normal in sulphuric acid. 7 p

For removal of the last part of the aluminum present. this mother liquor is concentrated .to a

. specific gravity of 1.32 at boiling temperature.

or to a volume of about 60 liters, and then crys- Society, 50, 1900 (1929)). It has a'specific gravity 01 about 1.30 at 20 C. and contains about:

73 grams BeO per liter and 10 grams FezO: per liter in the form of sulphates.

For separation of the beryllium from the iron the filtrate is concentrated to about 1.45-1.46 specific gravity at boiling temperature, and the solution crystallized by cooling, having preferably first reduced the iron with sulphur dioxide. The

crystals formed contain .01% 02 F620;. By recrystallization of the beryllium sulphate formed the iron content of the crystals is only .002 to 003%. In other words, the beryllium sulphate is practically chemically pure.

It will be understood that the beryllium sulphate produced can be treated in various known. ways to convert the beryllium content to difi'erent forms. For example, the sulphate'can be converted to beryllium oxide by heating it to drive oflf sulphur trioxidegand the beryllium oxide, in turn, can be converted into various other compounds such as fluorides and chlorides suitable for electrolysis.

As further illustrating the practice 01 our improved process, we give the following example using hydrochloric acid as reagent:

A suitable amount of beryl modified, as previously explained, by melting and quenching and ground to pass a 200- mesh sieve, is mixed with concentrated hydrochloric acid largely in excess of the amount theoretically necessary to react with the silicates oi the ore. We have found that an excess of 100% is suitable which is equivalent to a ratio of 4 cc. of the concentrated acid to one gram of beryl like that of the first example above given.

The mixed beryl and acid when heated react to form a solution of beryllium, aluminum and iron chlorides and with the heating conducted at 84 C. for about 19 hours the yield of beryllium chloride is approximately 66% and of the aluminum and iron chlorides combined approximately 67%. v

The separation 01' the chlorides'is effected by treatment or the solution in known ways. For example, the solution can be treated with hydrochioric acid gas at low temperatures to effect with oxides of alkalis and alkaline earths and with magnesium oxide lnorder to decompose the beryl andrender the iormed materials soluble in sulphuric acid. It is also known to sinter or i'use aluminum silicates containing considerable amounts of alkalis, such as feldspar, in order to render them soluble in sulphuric acid. Furthermore, it is known to heat aluminum ores, such as clay, to temperatures below 900 C. to render them more reactive to sulphuric acid. However, the present process is distinguished in that the heat treatment increases thereactivity oi the beryl to reagents, such as sulphuric acid, by effecting a change in the physical structure oi the ore and without any substantial change in crease in reactivity is secured in an ore which contains no significant amount of alkalis. The result, in the present process, is to make the ore beryl, heretofore considered highly resistant, subject to direct attack by reagents, such as sulphuric acid, which would not attack the natural its chemical composition, and in that this instantial change in its chemical composition, it is to be observed that water of crystallization present in the ore may be driven off by the modifying" treatment so that it would perhaps be more accurate to say that the present process changes the internal physical structure of the ore while substantially maintaining its original chemical com position with respect to beryllium oxide,alumina and silica. However, since raw beryl ordinarily contains very little water of crystallization it seems proper to say that no substantial change in its chemical composition results from drivin off its water of crystallization.

The present application constitutes a continuation in .part ofour earlier filed applications Serial No. 5,169, filed January 27, 1925, and Serial No. 123,593, filed July 19, 1926. In the present application we do not claim the herein disclosed methods of recovering the beryllium and aluminum from the ore after it has been treated with sulphuric acid or other reagent, these several methods or features and certain features incidentalthereto being claimed in our copcnding application Serial No. 536,518, filed May 11, 1931, as a division of the present application.

To those skilled in the art it will be apparent that our invention can be practiced with a variety of modifications and in various differing embodiments without departing from the spirit and scope thereof as defined in the appended claims. It will also be understood that the modified beryl produced by our process is a product which can be utilized in various ways to take advantage.

of its novel physical and chemical characteristics.

What we claim is:

l. The process of extracting beryllium from beryl which consists in increasing the chemical reactivity of the beryl by heating it above 1000' C. under conditions which change its original physical structure and substantially maintain its original chemical composition with respect to BeO, A1202, and S102 and cooling it, and thereafter treating the modified beryl with a reagent at temperatures adaptedto transform beryllium content thereof directly into a soluble forml 2. The process of extracting beryllium from beryl which consists in increasing the chemical reactivity of the beryl by heating it above 1000' C. under conditions which change its original physical structure and substantially maintain its original chemical composition with respect to BeO, A1203, and S102 and cooling it, and thereafter treating the modified beryl with a mineral acid of a temperature and a concentration adapted to transform beryllium content of the beryl directly into a soluble form.

3. Theprocess of extracting beryllium from beryl' which consists in increasing the'chemical reactivity of the beryl by heating it above 1000 C. under conditions which change its original physical structure and substantially its original chemical composition with respect to BeO, A1201, and S102 and cooling it, and thereafter treating the modified beryl with sulphuric acid of a temperature and concentration adapted to transform beryllium content of the beryl directly into beryllium sulphate.

4. The process of extracting beryllium from beryl which consists in increasing the chemical reactivity of the beryl by heating it above 1000 C. under conditions which change its original 2 physical structure and substantially maintain its orlginal chemical composition with respect to BeO, A:. and S102. rapidly cooling the heated material to fix its changed physical structure,

and thereafter treating the modified beryl with a mineral acid of a temperature and concentration adapted to transform beryllium content of the beryl directly into a soluble form.

5. The process of extracting beryllium from after treating the said material with a miner-i acid of a temperature and concentration adapted to transform beryllium content of the beryl directly into a soluble form.

' 6.-The process of extracting, beryllium from beryl whichconsists in increasing the chemical reactivity of the beryl by heating it to a molten state under conditions which change its original physical structure and substantially maintain its original chemical composition with respect, to BeO, A120:, and S102, rapidly cooling the melted material to fix its modified structure, and thereafter treating the said material with sulphuric acid of a temperature and concentration adapted to transform beryllium content of the beryl directly into beryllium sulphate.

its internal physical structure and cooling the molten material by quenching.

9. The process of extracting beryllium from beryl which consists in increasing the chemical reactivity of the beryl by heating it above 1000? C. under conditions which change its original physical structure and substantially maintain its original chemical composition with respect to BeO, A1202, and Si02, cooling the heated material, and treatingthe said material in a closed con tainer with a reagent at a temperature and concentration adapted to produce superatmospheric pressure in the container and to transform berylllum content of the said material directly into soluble form. I r

10. The process of extracting beryllium from beryl which consists in increasing the chemical reactivity of the beryl by heating it above 1000" 'C. under conditions which change its original physical structure and substantially maintain its original chemical composition with respect to BeO, A120:, and S102, cooling the heatedmaterial, and treating the said material in a closed container with a mineral acid at a temperature and concentration adapted to produce superatmospheric pressure in the container and to transberyl which consists in increasing the chemical andtreatingthesaidmaterialinaclosedcon-u tainer with sulphuric acid at a temperature and concentrationadapted to produce superatmospheric pressure in the container and to transform beryllium content of the said material directly into beryllium sulphate.

12. In a process of extracting beryllium from beryl, the step which consists in treating the beryl in a closed container with sulphuric acid at a temperature and concentration adapted to produce superatrnospheric pressure in the container and to transform beryllium content of the beryl into beryllium sulphate.

13. The process of increasing the susceptibility oi beryl to the subsequent action or axchemical reagent, which process consists in a thermal treatment of the beryl above 1000 C. under conditions which change its original physical structure and substantially maintain its original chemical composition with respect to BeO, A1201, and S102,

and rapidly cooling the beryl from its heated state.

14. As a new and useiful product, a substance produced by treating raw beryl as defined in claim 7, said substance having substantially the original chemical composition of the raw beryl with respect to BeO, A1101, and S102, and a chemical reactivity to sulphuric acid that is substantially greater than that of the raw beryl. 

